Jaime Fernandez-Sanchez, Ana Cuesta, Shiva Shirani, Cinthya Redondo-Soto, Angeles G De la Torre, Isabel Santacruz, Ines R Salcedo, Laura Leon-Reina, Miguel A G Aranda
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Data are sequentially acquired by Mo <i>K</i>α<sub>1</sub> laboratory X-ray powder diffraction (LXRPD) and microtomography (µCT), where the same volume is scanned with time to reduce variability. Wide capillaries (2 mm in diameter) are key to avoid artefacts, <i>e.g.</i> self-desiccation, and to have excellent particle averaging. This methodology is tested in three cement paste samples: (i) a commercial PC 52.5 R, (ii) a blend of 80 wt% of this PC and 20 wt% quartz, to simulate an addition of supplementary cementitious materials, and (iii) a blend of 80 wt% PC and 20 wt% limestone, to simulate a limestone Portland cement. LXRPD data are acquired at 3 h and 1, 3, 7 and 28 days, and µCT data are collected at 12 h and 1, 3, 7 and 28 days. Later age data can also be easily acquired. In this methodology, the amounts of the crystalline phases are directly obtained from Rietveld analysis and the amorphous phase contents are obtained from mass-balance calculations. From the µCT study, and within the attained spatial resolution, three components (porosity, hydrated products and unhydrated cement particles) are determined. The analyses quantitatively demonstrate the filler effect of quartz and limestone in the hydration of alite and the calcium aluminate phases. Further hydration details are discussed.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":null,"pages":null},"PeriodicalIF":6.1000,"publicationDate":"2024-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11299602/pdf/","citationCount":"0","resultStr":"{\"title\":\"Mix and measure II: joint high-energy laboratory powder diffraction and microtomography for cement hydration studies.\",\"authors\":\"Jaime Fernandez-Sanchez, Ana Cuesta, Shiva Shirani, Cinthya Redondo-Soto, Angeles G De la Torre, Isabel Santacruz, Ines R Salcedo, Laura Leon-Reina, Miguel A G Aranda\",\"doi\":\"10.1107/S1600576724004527\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Portland cements (PCs) and cement blends are multiphase materials of different fineness, and quantitatively analysing their hydration pathways is very challenging. 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引用次数: 0
摘要
硅酸盐水泥(PCs)和水泥混合料是不同细度的多相材料,对其水化途径进行定量分析非常具有挑战性。必须确定初始结晶相和无定形相的溶解(水化)情况,以及易溶组分(如埃特林特)、活性组分(如波长石)和无定形组分(如硅酸钙水合物凝胶)的形成情况。还必须绘制出微观结构随水化时间的变化图。为了稳健而准确地解决这一问题,我们正在开发一种创新方法,该方法基于对浆料的原位测量,无需对样品进行任何调节。通过 Mo Kα1 实验室 X 射线粉末衍射 (LXRPD) 和显微层析 (µCT) 顺序获取数据,在扫描过程中对同一体积进行扫描,以减少变化。宽毛细管(直径 2 毫米)是避免伪影(如自干燥)和获得优异颗粒平均性的关键。该方法在三种水泥浆样品中进行了测试:(i) 商品 PC 52.5 R,(ii) 80 wt% PC 和 20 wt% 石英的混合料,用于模拟添加胶凝补充材料,以及 (iii) 80 wt% PC 和 20 wt% 石灰石的混合料,用于模拟石灰石波特兰水泥。在 3 小时和 1、3、7 和 28 天时采集 LXRPD 数据,在 12 小时和 1、3、7 和 28 天时采集 µCT 数据。后期龄期数据也可轻松获取。在这种方法中,结晶相的数量可直接通过里特维尔德分析法获得,而非晶相的含量则可通过质量平衡计算获得。通过 µCT 研究,在达到的空间分辨率范围内,可以确定三种成分(孔隙率、水化产物和未水化水泥颗粒)。分析从数量上证明了石英和石灰石在水合铝土矿和铝酸钙相中的填充作用。还讨论了进一步的水化细节。
Mix and measure II: joint high-energy laboratory powder diffraction and microtomography for cement hydration studies.
Portland cements (PCs) and cement blends are multiphase materials of different fineness, and quantitatively analysing their hydration pathways is very challenging. The dissolution (hydration) of the initial crystalline and amorphous phases must be determined, as well as the formation of labile (such as ettringite), reactive (such as portlandite) and amorphous (such as calcium silicate hydrate gel) components. The microstructural changes with hydration time must also be mapped out. To address this robustly and accurately, an innovative approach is being developed based on in situ measurements of pastes without any sample conditioning. Data are sequentially acquired by Mo Kα1 laboratory X-ray powder diffraction (LXRPD) and microtomography (µCT), where the same volume is scanned with time to reduce variability. Wide capillaries (2 mm in diameter) are key to avoid artefacts, e.g. self-desiccation, and to have excellent particle averaging. This methodology is tested in three cement paste samples: (i) a commercial PC 52.5 R, (ii) a blend of 80 wt% of this PC and 20 wt% quartz, to simulate an addition of supplementary cementitious materials, and (iii) a blend of 80 wt% PC and 20 wt% limestone, to simulate a limestone Portland cement. LXRPD data are acquired at 3 h and 1, 3, 7 and 28 days, and µCT data are collected at 12 h and 1, 3, 7 and 28 days. Later age data can also be easily acquired. In this methodology, the amounts of the crystalline phases are directly obtained from Rietveld analysis and the amorphous phase contents are obtained from mass-balance calculations. From the µCT study, and within the attained spatial resolution, three components (porosity, hydrated products and unhydrated cement particles) are determined. The analyses quantitatively demonstrate the filler effect of quartz and limestone in the hydration of alite and the calcium aluminate phases. Further hydration details are discussed.
期刊介绍:
Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.